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Carbonate Ion → HCID 118105693, Verbindung

HRID 1496959
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1496959
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:3]=1.[C:18]([N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1)([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].C(=O)([O-])[O-]>CN(C)C=O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:28]2[CH2:27][CH2:26][N:25]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:30][CH2:29]2)=[CH:3][C:4]=1[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([O-:10])=[O:9]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 19660Carbonate IonHCID 143452tert-Butyl piperazine-1-carboxylateHCID 122900444-Chloro-1-nitro-2-phenoxybenzene

Produkt 1

HCID 118105693HCID 118105693, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

The compound (500 mg) prepared in Step 1, N-Boc-piperazine (500 mg) and tassium carbonate (2.0 g) were dissolved in dimethylformamide (3 ml), and stirred at 90° C. for 2 hours. The dimethylformamide of the mixed solution was removed by distillation under reduced pressure, and extracted with ethyl acetate. The extracted organic layer was washed with saturated brine, and water was removed with sodium sulfate, and the solvent was removed by distillation under reduced pressure. The solvent-removed mixture was purified by column chromatography to obtain a yellow target compound.

Aufarbeitung

  1. customThe dimethylformamide of the mixed solution was removed by distillation under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe extracted organic layer was washed with saturated brine, and water
  4. customwas removed with sodium sulfate
  5. customthe solvent was removed by distillation under reduced pressure
  6. customThe solvent-removed mixture was purified by column chromatography
  7. customto obtain a yellow target compound

Quellen und Nachweise

ORD-Eintrag
ord-d2edc7c56d704cd9930c1dfb79e3bcce
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09199944B2

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